CN110713716A - High-thermal-conductivity polydopamine modified boron nitride/polyimide composite material and preparation method thereof - Google Patents
High-thermal-conductivity polydopamine modified boron nitride/polyimide composite material and preparation method thereof Download PDFInfo
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- 229920001690 polydopamine Polymers 0.000 title claims abstract description 83
- 239000004642 Polyimide Substances 0.000 title claims abstract description 53
- 229920001721 polyimide Polymers 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical class N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 28
- 238000000967 suction filtration Methods 0.000 claims abstract description 15
- 238000007731 hot pressing Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 13
- 229940113088 dimethylacetamide Drugs 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
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- 238000005507 spraying Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
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- 239000004416 thermosoftening plastic Substances 0.000 claims description 2
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- 238000009736 wetting Methods 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims 1
- 239000008188 pellet Substances 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 2
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- 230000000052 comparative effect Effects 0.000 description 8
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- 229920000642 polymer Polymers 0.000 description 6
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- 229910003475 inorganic filler Inorganic materials 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 3
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
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- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229920004747 ULTEM® 1000 Polymers 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K9/10—Encapsulated ingredients
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- C08K3/38—Boron-containing compounds
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- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The specification discloses a high-thermal-conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material and a preparation method thereof, and belongs to the field of preparation of high-performance thermal-conductivity composite materials, the composite material comprises two components, namely polyimide (PI, 68.9 ~ 91.3.3 wt%) and polydopamine modified boron nitride (BN @ PDA, 8.7 ~ 31.1.1 wt%), the content of PDA in the modified filler BN @ PDA is 1.46 wt%, BN is coated with PDA to obtain the modified filler BN @ PDA, the modified filler BN @ PDA is blended with a PI solution, the interface between the modified filler BN @ PDA and PI can be improved by introducing a hydrogen bond, agglomeration is inhibited, the interface thermal resistance is reduced, a blank with BN @ PDA highly oriented in the surface of a PI matrix is prepared by vacuum-assisted suction filtration, and then the composite material is formed by hot pressing at a proper temperature and a proper pressure, the defects of the composite material can be reduced, the in-plane orientation degree of the BN @ PDA in the PI matrix can be further improved, and the composite material is endowed with excellent in-plane thermal conductivity.
Description
Technical Field
The invention relates to a polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material with low interface thermal resistance and high orientation in a filler surface and a preparation method thereof, which are prepared by the processes of filler surface modification, vacuum-assisted suction filtration and hot press molding, so that the BN @ PDA/PI composite material is endowed with high heat-conducting property. This patent belongs to high performance heat conduction composite preparation field.
Background
With the development of modern electronic equipment towards miniaturization, integration and multi-functionalization, if heat generated in the operation process is difficult to discharge in time, the local temperature of the equipment is too high, and the reliability and the service life of the equipment are seriously influenced. Polyimide (PI) has the advantages of aging resistance, high and low temperature resistance, high mechanical property and the like, and is widely applied to the fields of aerospace, electronic devices and the like. However, PI has a low intrinsic thermal conductivity (< 0.4W/(m · K)), which limits its application as a thermal conductive material in the field of electronic devices.
In order to increase the thermal conductivity of the polymer, a method of introducing a highly thermally conductive inorganic filler into a polymer matrix is generally employed. However, inorganic fillers introduce factors that are detrimental to the thermal conductivity. On one hand, the inorganic filler is not easy to be uniformly dispersed in the polymer; on the other hand, a large amount of interfaces can be introduced due to poor compatibility of the inorganic filler and the polymer. The literature reports that by surface modification of fillers, for example: the above problems can be overcome by introducing hydrogen bonds, reactive functional groups, filler bridging, and the like. Boron Nitride (BN), one of the high-thermal-conductivity fillers, is relatively inert on the surface, and the heat conductivity of the composite material is limited by adopting a general silane coupling agent to treat the BN.
Dopamine can be polymerized on the solid surface to form Polydopamine (PDA), has universal adhesion capability, and a large number of amino groups and hydroxyl groups are introduced to form hydrogen bonds with the polymer, so that the problem of poor compatibility between the filler and the polymer interface can be greatly improved, and the interface thermal resistance is reduced. Chinese patent CN105647015A discloses a polypropylene composite material with high thermal conductivity and a preparation method thereof. The dopamine modified boron nitride/polypropylene composite material is prepared by adopting a melt blending and injection molding method, and the thermal conductivity of the filler containing 25 wt% and 50 wt% of the filler respectively reaches 4.94W/(m.K) and 7.92W/(m.K). However, polypropylene, as a general-purpose plastic, cannot be applied to many occasions with high requirements on thermal properties, mechanical properties and the like.
According to the preparation method, the high-heat-conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material with excellent mechanical properties and strong practicability is prepared by coating BN with PDA, blending with PI and a solvent (DMAc) and then performing a processing process combining vacuum-assisted suction filtration and hot pressing. When the mass part of the filler is 31.1 parts, the thermal conductivity of the BN @ PDA/PI composite material can be as high as 3.01W/(m.K). Through research on relevant documents and patents, reports of the high-thermal-conductivity BN @ PDA/PI composite material which is the same as or similar to the patent and a preparation method thereof are not found.
Disclosure of Invention
The invention aims to provide a PI-based composite material with high thermal conductivity and excellent mechanical properties, and the specific technical scheme is as follows:
a high-thermal-conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material comprises two components, namely polyimide (PI, 68.9 ~ 91.3.3 wt%) and polydopamine modified boron nitride (BN @ PDA, 8.7 ~ 31.1.1 wt%), wherein the content of PDA in modified filler BN @ PDA is 1.46 wt%, BN is coated by PDA, the modified filler BN @ PDA is blended with PI and a solvent (DMAc), and then the BN @ PDA/PI composite material is prepared through vacuum-assisted suction filtration and hot pressing.
The preparation method comprises the following steps:
(1) the BN @ PDA is prepared by dispersing BN powder in deionized water, adding a certain amount of tris (hydroxymethyl) aminomethane, sequentially adding a certain amount of ethanol and hydrochloric acid solution (0.1 mol/L) after completely dissolving, uniformly stirring, finally adding a proper amount of dopamine hydrochloride, stirring for 5 ~ 10h, centrifugally washing the obtained BN @ PDA dispersion liquid for 3 ~ 5 times by using ethanol/water mixed liquid at the rotating speed of 3000 ~ 5000 rpm, carrying out suction filtration, and drying at 60 ~ 80 ℃ for 10 ~ 16 h to obtain the BN @ PDA modified filler, wherein the deionized water, the tris (hydroxymethyl) aminomethane, the ethanol, the hydrochloric acid solution, the dopamine hydrochloride = 4g, 260 mL, 10mmol, 100 mL, 40 mL and 640 mg are adopted.
(2) Preparing PI solution by adding PI raw material into certain amount of dimethyl acetamide (DMAc), stirring at 120 ~ 140 deg.C for 6 ~ 10h, and setting the solid content of PI solution at 25 ~ 30%;
(3) and (2) preparing a mixed solution of BN @ PDA/PI, namely mixing BN @ PDA with DMAc in a certain mass, sequentially carrying out ultrasonic treatment for 20 ~ 40min, mixing the mixed solution with a proper amount of PI solution, and stirring for 20 ~ 40min, wherein the mass ratio of the PI to the DMAc in the mixed solution of BN @ PDA/PI is 1: 4.
(4) Preparing a sample blank by vacuum-assisted suction filtration, namely filling slow-speed qualitative filter paper into a Buchner funnel, wetting the filter paper by deionized water, quickly opening a vacuum pump to drain excessive water, but keeping the filter paper wet, extracting a proper amount of mixed liquid, uniformly coating the mixed liquid on the filter paper without a gap with the inner wall of the funnel, opening the vacuum pump to carry out suction filtration for 4 ~ 6 h, peeling a sample from the filter paper, heating the sample to 180 ℃ from room temperature within 10 ~ 15 h in a blast oven, and then preserving heat for 1 ~ 2 h for drying;
(5) and (3) preparing the high-thermal-conductivity composite material by hot pressing, namely spraying a release agent on an upper template and a lower template, placing the blank between the templates, placing the blank in a flat vulcanizing machine at the temperature of 230 ~ 250 ℃, preheating for 5 ~ 10 min, and hot pressing for 10 ~ 15min under the pressure of 10 ~ 20 MPa to obtain a product.
The method comprises the steps of firstly coating BN by using PDA to obtain BN @ PDA filler, improving the interface between the BN @ PDA filler and a PI substrate by introducing a hydrogen bond, and reducing the interface thermal resistance; then, preparing a BN @ PDA highly oriented blank in the surface of the PI matrix by vacuum-assisted suction filtration; and then, hot-pressing the mixture into a composite material at a proper temperature and under proper pressure, so that the defects of the composite material are reduced, the orientation degree of BN @ PDA in the PI matrix plane is further improved, and finally the composite material is endowed with excellent in-plane heat-conducting property.
In the preparation method of the BN @ PDA/PI composite material, the PI raw material is soluble thermoplastic PI granules.
In the preparation method of the BN @ PDA/PI composite material, the BN raw material is BN powder with the average size of 30 mu m.
The thermal conductivity of the samples prepared according to the invention was measured at room temperature using a Hot Disk thermal constant analyzer. The test results show that when the coating amount of PDA is 1.46 wt% and the mass part of BN @ PDA is 31.1 parts (example 4), the thermal conductivity is as high as 3.01W/(m.K), which is 15 times higher than that of pure PI (comparative example 5), and is improved by 0.66W/(m.K) compared with the composite material without PDA modification (comparative example 4). Meanwhile, the composite material prepared by the method has excellent mechanical property and can be recovered after being bent at a large angle. The method is a preparation method of the PI-based composite material with high thermal conductivity, which has a very good application prospect and practicability.
In addition, the invention also has the following advantages:
1) the components of the composite material are simple, the selected raw materials are commercial products, and the in-plane thermal conductivity of the composite material can be remarkably improved at a lower BN addition amount.
2) The equipment of the patent is simple, and only common equipment such as a vacuum pump, a hydraulic press and the like is used.
3) The method is easy to implement, simple in equipment maintenance and cleaning and free of harsh requirements on environmental conditions.
Drawings
FIG. 1 shows SEM and numerical (upper right corner of picture) pictures of BN (a), BN @ PDA (b). The BN after PDA modification is changed from white to brown, which indicates that the BN (white) microchip is coated with the PDA (brown).
FIG. 2 is a cross-sectional photograph of example 4, which shows that the BN filler is highly oriented in the plane, and the filler are mutually overlapped to form a perfect heat conduction path.
FIG. 3 (a) is a graph showing the change in tensile strength of example 1 ~ 4 and comparative examples 2, 4 and 5, and (b) is a graph showing the bending of the composite material of example 4.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following examples are given to illustrate the present invention and it should be noted that the following examples are only for illustrative purposes and should not be construed as limiting the scope of the present invention, and the non-essential modifications and variations of the present invention by those skilled in the art according to the above disclosure will still fall within the scope of the present invention.
Example 1 ~ 4 and comparative example 1 ~ 5:
(1) preparation of BN @ PDA: 4g of BN (BBN-30, a product of Yaanbai high-new material Co., Ltd.) powder is dispersed in 260 mL of deionized water, 10mmol (1.2114 g) of tris (hydroxymethyl) aminomethane is added, after complete dissolution, 100 mL of absolute ethanol and 40 mL of hydrochloric acid (0.1 mol/L) are sequentially added while stirring, and finally 640 mg of dopamine hydrochloride is added, and magnetic stirring is carried out for 6 hours. The obtained BN @ PDA dispersion was washed by centrifugation 4 times with an ethanol/water mixture at 4000 rpm. After suction filtration, drying for 12 h at 70 ℃ to obtain BN @ PDA modified filler;
(2) preparation of PI solution: adding a PI raw material (Ultem 1000, a product of Sabour basic Innovation plastics Co., Ltd.) into a certain amount of DMAc, and magnetically stirring for 10 hours at 120 ℃ to obtain a PI solution with the solid content of 25%;
(3) preparation of BN @ PDA/PI/DMAC blend: mixing a certain mass of BN @ PDA (example) or BN (comparative example) with a certain amount of DMAc, sequentially carrying out ultrasonic treatment for 20 min, mixing the mixture with a proper amount of 25% PI solution, and carrying out magnetic stirring for 30 min. Comparative example the operations were the same as in example except that no PDA modification was performed. The specific formula is shown in the table I.
Table a formulation table of the suction filtration materials of examples 1 to 4 and comparative example 1 ~ 5.
Note: the composite material contains filler mass parts = pumping filtration material filler mass parts ÷ (PI solution mass parts × 25% + pumping filtration material filler mass parts) × 100.
(4) Preparing a sample blank by vacuum-assisted suction filtration: loading slow-setting filter paperΦWetting an 80mm specification Buchner funnel with deionized water, then quickly opening a vacuum pump to pump off excessive water, and still keeping filter paper wet; the mixture is extracted by a syringe with 10 mL and is evenly coated on filter paper without clearance with the inner wall of the funnel; after a vacuum pump is started for suction filtration for 5 hours, peeling a sample from filter paper, placing the sample in a blast oven, heating the sample to 180 ℃ from room temperature for 13 hours, and keeping the temperature for 1 hour for drying;
(5) preparing a highly-oriented high-thermal-conductivity composite material with a filler by a hot-pressing method: and (3) spraying a release agent on the upper template and the lower template, placing the blank between the templates, placing the blank in a flat vulcanizing machine at the temperature of 230 ℃, and sequentially preheating for 5min and hot-pressing for 10 min at 15 MPa to obtain the composite material with the thickness of about 300 mu m. The content of each component of the final sample is shown in table two, and the statistical table of the thermal conductivity of different composites is shown in table three.
Table two component content tables of examples 1 to 4 and comparative example 1 ~ 5.
Table three statistical tables of thermal conductivity of different PI/BN composites. Unit: W/(m.K)
Claims (7)
1. A high-thermal-conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material is characterized by comprising two components, namely polyimide (PI, 68.9 ~ 91.3.3 wt%) and polydopamine modified boron nitride (BN @ PDA, 8.7 ~ 31.1.1 wt%), wherein the content of PDA in the modified filler BN @ PDA is 1.46 wt%, BN is coated by PDA, then the modified filler BN @ PDA is mixed with PI and a solvent (DMAc), and then the mixed material is subjected to vacuum-assisted suction filtration, drying and hot pressing in sequence to obtain the BN @ PDA/PI composite material.
2. A preparation method of a high-thermal-conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material is characterized by comprising the following steps:
(1) the preparation of BN @ PDA comprises the steps of dispersing BN powder into deionized water, adding tris (hydroxymethyl) aminomethane, sequentially adding absolute ethyl alcohol and hydrochloric acid solution after complete dissolution, stirring uniformly, finally adding dopamine hydrochloride, stirring for 5 ~ 10h, centrifugally washing the obtained BN @ PDA dispersion liquid for 3 ~ 5 times by using ethanol/water mixed liquid, wherein the rotating speed is 3000 ~ 5000 rpm, carrying out suction filtration, and drying at 60 ~ 80 ℃ for 10 ~ 16 h to obtain BN @ PDA modified filler;
(2) the PI solution is prepared by adding PI raw material into dimethyl acetamide (DMAc), and stirring at 120 ~ 140 deg.C for 6 ~ 10 h;
(3) mixing BN @ PDA with DMAc, sequentially carrying out ultrasonic treatment for 20 ~ 40min, mixing the mixture with a PI solution, and stirring for 20 ~ 40min, wherein the mass ratio of PI to DMAc in the BN @ PDA/PI mixed solution is 1: 4;
(4) preparing a sample blank by vacuum-assisted suction filtration, namely filling slow-speed qualitative filter paper into a Buchner funnel, wetting the filter paper by deionized water, starting a vacuum pump to pump excessive water, but keeping the filter paper wet, pumping a proper amount of mixed liquid, uniformly coating the mixed liquid on the filter paper without a gap with the inner wall of the funnel, starting the vacuum pump to pump for 4 ~ 6 hours, peeling a sample from the filter paper, heating the sample to 180 ℃ from room temperature within 10 ~ 15 hours in a blast oven, and then preserving heat for 1 ~ 2 hours for drying;
(5) and (3) preparing the high-thermal-conductivity composite material by hot pressing, namely spraying a release agent on an upper template and a lower template, placing the blank between the templates, placing the blank in a flat vulcanizing machine at the temperature of 230 ~ 250 ℃, preheating for 5 ~ 10 min, and hot pressing for 10 ~ 15min under the pressure of 10 ~ 20 MPa to obtain a product.
3. The method for preparing high thermal conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material according to claim 2, wherein the PI raw material is soluble thermoplastic PI pellets.
4. The method for preparing high thermal conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material according to claim 2, wherein the BN raw material is BN powder with average size of 30 μm.
5. The method for preparing high thermal conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material according to claim 2, wherein the concentration of the hydrochloric acid solution used in the step (1) is 0.1 mol/L.
6. The preparation method of the high thermal conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material as claimed in claim 2, wherein in the step (1), the BN is deionized water, tris (hydroxymethyl) aminomethane, absolute ethyl alcohol, hydrochloric acid solution, dopamine hydrochloride = 4g, 260 mL, 10mmol, 100 mL, 40 mL and 640 mg.
7. The preparation method of the high thermal conductivity polydopamine modified boron nitride/polyimide (BN @ PDA/PI) composite material according to claim 2, wherein the solid content of the PI solution prepared in the step (2) is 25 ~ 30%.
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| CN114750491A (en) * | 2022-05-24 | 2022-07-15 | 陕西科技大学 | Polydopamine modified boron nitride nanosheet/polyimide heat-conducting and insulating composite film and preparation method and application thereof |
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